CN105061144B - Impurity removal method and impurity removal system for cationic dyeable polyester device - Google Patents
Impurity removal method and impurity removal system for cationic dyeable polyester device Download PDFInfo
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- CN105061144B CN105061144B CN201510503526.6A CN201510503526A CN105061144B CN 105061144 B CN105061144 B CN 105061144B CN 201510503526 A CN201510503526 A CN 201510503526A CN 105061144 B CN105061144 B CN 105061144B
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- ethylene glycol
- trash separator
- esterification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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Abstract
The invention relates to an impurity removal method for a cationic dyeable polyester device and an impurity removal system, adopting the impurity removal method, for the cationic dyeable polyester device. The impurity removal method comprises the following steps: secondary esterifiable mixed steam and ethylene glycol recycled for polycondensation are sent into impurity removal equipment for impurity removal, wherein a heating device is arranged on the impurity removal equipment; gas-phase water and gas-phase ethylene glycol are obtained through heating, and gather at the upper part in the inner cavity of the impurity removal equipment; oligomers and other impurities to be removed are liquid-phase and gather at the lower part in the inner cavity of the impurity removal equipment; a gas mixture of gas-phase water and gas-phase ethylene glycol is sent into a polyester process tower for separation of gas-phase water and gas-phase ethylene glycol; both the gas mixture and primary esterifiable mixed steam are subjected to the separation of gas-phase water and gas-phase ethylene glycol in the polyester process tower. The impurity removal system comprises the impurity removal equipment and the polyester process tower, wherein an impurity removal equipment reboiler is arranged on the impurity removal equipment reboiler. Compared with the conventional impurity removal process, the impurity removal method and the impurity removal device provided by the invention have the advantages that the process concept is innovated; under the premise that the purpose of impurity removal is fulfilled, the structure of the impurity removal equipment is simplified, the energy consumption is reduced, the adverse impact on a reactor is avoided, and the guarantee of product quality is facilitated.
Description
Technical field
The present invention relates to a kind of impurity-removing method of cation dyeable polyester device, further relate to a kind of sun of employing the method from
The impurity removed system of sub- dyeable polyester device, is mainly used in mixing the second esterifier generation in cation dyeable polyester device
What conjunction steam and polycondensation unit were produced carries out remove impurity containing water glycol, removes oligomer contained therein and other impurities, improves sun
The product quality of ion dyeable polyester, and obtain the ethylene glycol of reusable edible.
Background technology
Cation dyeable polyester device is mainly made up of esterification unit and polycondensation unit, raw material PTA (refined terephthaldehydes
Acid) and EG (ethylene glycol) through esterification and polycondensation after, formation PET（Polyethylene terephthalate, may be simply referred to as polyester）, lead to
Often esterification unit is made up of the first esterifier and the second esterifier, and is added for reality in the second esterifier
Three monomers of existing cationic dye capable of dyeing（Such as 5- sodium sulfonates -1.3- M-phthalic acid hydroxyethyl esters, SIPE）Even four
Monomer etc., the addition of these raw materials makes course of reaction more complicated, and side reaction is relatively more, a part of oligomer and other
Impurity will be entrained with from the gas phase mixture of the second esterifier and the polycondensation reactor of postorder and, wherein the second esterification
Mixed vapour in addition to the ethylene glycol for mainly including, also comprising less than the water of 10wt%, a small amount of diethylene glycol and acetaldehyde and a small amount of oligomeric
Thing, is condensed in the reuse ethylene glycol for being formed in addition to the ethylene glycol for mainly including by the mixed vapour of polycondensation reaction, also including～
The water of 3wt%, a small amount of diethylene glycol and oligomer and micro acetaldehyde.
For the reuse of this ethylene glycol containing impurity such as oligomer, there are two kinds of technology paths, a part of device at present
By being separately provided purifying ethylene glycol system（Mainly it is made up of independent purifying ethylene glycol Tower System）, remove impurity therein and
Ethylene glycol is back to into esterification unit after water；A part of device is then not provided with purifying ethylene glycol system, but as the first esterification
Mixed vapour equally send into polyester process tower（EG/H2O knockout towers）, it is separated only by out ethylene glycol reuse after water therein just
In esterification unit.By contrast, using the product of the cation dyeable polyester prepared after independent purifying ethylene glycol Tower System
Quality is better, but energy consumption also can be higher（Energy consumption about increases by 19.2%）, and do not set independent purifying ethylene glycol Tower System
, the product quality of the cation dyeable polyester prepared relatively almost, and due in system oligomer and impurity in pipeline
Middle circulation and accumulation, pipeline is easily blocked, and overhauls related frequency, and the production dedoping step of cation dyeable polyester still very must
Want.
At present, for the second esterification the purifying ethylene glycol tower bag that mixed vapour and the reuse ethylene glycol of polycondensation reaction is arranged
Tower reactor and the respectively tower body and reboiler of self-corresponding opening UNICOM each with tower reactor top are included, the bottom of tower reactor is provided with tower bottoms
Extraction mouth, tower bottoms extraction mouth be connected with the tube side inlet of reboiler, tower body be provided with after refined material inlet with refine after thing
Material outlet, tower reactor is sent into using the reuse ethylene glycol of the mixed vapour of the second esterification and the polycondensation reaction as material to be refined
Afterwards, steam is refined into tower body, and heavy constituent and reuse ethylene glycol collect in tower reactor, and the discharging of Jing tower reactors is pumped to reboiler
Heating, unevaporated heavy constituent flows back to tower reactor, and the light component for evaporating is refined at the top of tower reactor into tower body, in tower reactor
Heavy constituent viscosity is continuously increased, and the liquid in tower reactor is drained into waste collection groove by interval.Ethylene glycol after tower body is refined
Produced by the ethylene glycol side take-off mouth in the middle part of tower body, the light component such as vapor is steamed by tower body top exit and enters overhead condensation
Simultaneously part is back to tower body by tower body upper return mouth for device condensation, and reflux ratio is 8～10.
The defect of above-mentioned impurity removing technology is mainly manifested in：First, the reflux ratio that this method needs is higher, is 8～10, because
This energy consumption is larger, and should arrange special tower body and overhead condensate reflux system also increases equipment investment.Secondly, sun from
In the continuous production of sub- dyeable polyester, because the addition of three monomers, oligomer viscosities are larger in the mixed vapour of the second esterification, tower
Kettle liquid body needs frequent intermittent to discharge, thus quantity of steam frequently has greatly changed in tower so that the operating pressure of tower is very
It is unstable, it is not easy to operate.Again, the pressure change of tower can affect the pressure in the second esterifier for being attached thereto again, instead
Answer the change of pressure in device has detrimental effect to the quality of esterification products.
The content of the invention
In order to overcome the drawbacks described above of prior art, the invention provides a kind of remove impurity side of cation dyeable polyester device
Method and a kind of knot screen of the cation dyeable polyester device of employing the method, while remove impurity purpose is realized, to simplify
The device structure of remove impurity, reducing energy consumption, and the adverse effect to reactor is avoided, advantageously ensure that product quality.
The technical solution adopted in the present invention is：
A kind of impurity-removing method of cation dyeable polyester device, by the mixed vapour of the second esterification and the reuse of polycondensation reaction
Ethylene glycol sends into trash separator remove impurity, and the trash separator is not provided with for entering water-filling and the detached independent knockout tower of ethylene glycol, only
Use equivalent to a vaporizer, heating makes water and ethylene glycol be gas phase and be gathered in the top of trash separator inner chamber, poly- sending into
Water and ethylene glycol gaseous mixture before ester process tower not to being formed enters water-filling and the separation of ethylene glycol, and oligomer is wanted with other
The impurity of removing is liquid phase and is gathered in the bottom of trash separator inner chamber, and then trash separator is discharged by way of accomplished continuously or intermittently,
Water and ethylene glycol gaseous mixture are sent into for water and the detached polyester process tower of ethylene glycol, are being gathered with the mixed vapour of the first esterification
Enter the light component such as water-filling and the separation of ethylene glycol, water and acetaldehyde impurity in ester process tower to be steamed by the tower top of polyester process tower, liquid
The ethylene glycol of phase is produced from the bottom of towe of polyester process tower, used as the refined ethylene glycol for being back to esterifier.
The trash separator can adopt the remove impurity kettle of autoclave structure and be provided with trash separator reboiler, by trash separator reboiler
To liquid phase heating evaporation again, water and ethylene glycol contained therein is further vaporized with.
Ethylene glycol spray can be carried out to the water of trash separator top output and ethylene glycol gaseous mixture, trap three for wherein carrying secretly
Monomer and other impurities.
Ethylene glycol for ethylene glycol spray can be the reuse ethylene glycol of polycondensation reaction, and the liquid phase after spray flows into remove impurity
Device.
When trash separator adopts intermittent mode deslagging, the liquid level or temperature of trash separator can be come by the heat source of trash separator
Control, for example, the liquid level of trash separator is controlled using the flow of the primary fluid for trash separator heating, or using for remove impurity
The primary fluid flow of device heating so as to realize the relatively stable of trash separator liquid level, is realized realizing the heating curve of trash separator
The stable operation of impurity removed system.
When trash separator adopts continuation mode deslagging, the liquid level of trash separator can be controlled by deslagging flow, trash separator
Operation temperature can be controlled by heat source, for example, control to remove using the flow of the primary fluid for trash separator heating
The temperature of miscellaneous device, so as to realize the stable operation of impurity removed system.
A kind of knot screen of cation dyeable polyester device, including trash separator and for water and the detached polyester of ethylene glycol
Process tower, the trash separator is not provided with for water and the detached independent separate tower of ethylene glycol, is just corresponded to a vaporizer and is used,
The mixed vapour output channel of the esterification of trash separator connection second and the reuse ethylene glycol output channel of polycondensation reaction, thus connect
Enter the mixed vapour of the second esterification and the reuse ethylene glycol of polycondensation reaction and carry out heating evaporation so as in water and ethylene glycol be
Gas phase, is gathered in the top of trash separator inner chamber, and oligomer and other impurity that should be removed are liquid phase and are gathered in trash separator inner chamber
Bottom, be provided with mixed gas outlet at the top of the trash separator, bottom is provided with slag-drip opening, and the polyester process tower connects the first ester
The mixed vapour output channel of change and the mixed gas outlet of the trash separator, the mixed vapour and trash separator for accessing the first esterification is defeated
The water for going out and ethylene glycol gaseous mixture simultaneously carry out heating evaporation so as in water and the light component impurity such as acetaldehyde be gas phase, ethylene glycol
For liquid phase, the tower top of the polyester process tower is provided with steam outlet, and bottom of towe is provided with refined ethylene glycol outlet.
The trash separator can adopt the remove impurity kettle of autoclave structure and can be provided with trash separator reboiler, and the trash separator is again
Boiling device is located at the top of the trash separator, and its top is provided with material inlet, and the bottom of the trash separator is provided with material outlet, described
The material outlet of trash separator reboiler directly connects the inner chamber of the trash separator, institute by the respective openings at the top of the trash separator
The material inlet for stating trash separator reboiler connects the slag-drip opening of the trash separator by trash separator circulating line, and the trash separator is followed
Endless tube road is provided with trash separator circulating pump.
Trash separator circulation between the material inlet of the trash separator circulating pump and the trash separator reboiler
Waste liquid extraction pipe can be connected with pipeline, waste collection groove is accessed in the outer end of the waste liquid extraction pipe, with periodically by trash separator
The excessive liquid phase of middle viscosity enters the waste collection groove.
Ethylene glycol spray device can be provided with the mixed gas outlet of the trash separator, the ethylene glycol spray device is provided with
Shower with nozzle, the injection direction of the nozzle is preferably inversely（With water and the outflow direction phase of ethylene glycol gaseous mixture
Instead）.
The shower can connect the reuse ethylene glycol output channel of the polycondensation reaction, with the reuse second of polycondensation reaction
Glycol as spray ethylene glycol and thus constitute the reuse ethylene glycol outlet tube that the trash separator connects the polycondensation reaction
A kind of mode in road.
The side of the trash separator can be provided with reuse ethylene glycol import, and the reuse ethylene glycol import connects the polycondensation
The reuse ethylene glycol output channel of reaction is simultaneously provided with regulating valve, thus constitutes the reuse that the trash separator connects the polycondensation reaction
The another way of ethylene glycol output channel.
The trash separator can be provided with external heater, it is also possible to be provided with built-in heater, the heater
It is provided with primary fluid conveyance conduit.
This knot screen is also provided with impurity removed system controller.
The trash separator can be provided with liquid level sensor and/or temperature sensor, and the liquid level sensor and/or temperature are passed
The signal output of sensor accesses the impurity removed system controller, the waste liquid extraction pipe or trash separator by wired or wireless way
Circulating line is provided with deslagging effusion meter, and the signal output of the deslagging effusion meter accesses remove impurity system by wired or wireless way
System controller, the primary fluid conveyance conduit is provided with primary fluid regulating valve, the corresponding control of the impurity removed system controller
Signal processed is input into respectively the control end of the primary fluid regulating valve and the trash separator circulating pump.
The invention has the beneficial effects as follows：Because the trash separator reboiler that connected using trash separator and its top is effectively by the
The light components such as the heavy constituents such as the oligomer in the mixed vapour of class generation and ethylene glycol, water are separated, then by light component steam
Deliver to polyester process tower carries out the refined of ethylene glycol together with the mixed vapour of the first esterification, goes the light components such as eliminating water, shape
Into refined ethylene glycol meet the prescription of esterification, can be with direct reuse in esterification unit；Due in trash separator
On be not provided with treating column, but the water produced after remove impurity and ethylene glycol gaseous mixture are sent directly into into polyester process tower and the first esterification
Mixed vapour together carry out purifying ethylene glycol, thus significantly simplify the structure of integral device, reduce equipment cost and
The space hold of equipment, while using polyester process tower feature, by the reflux ratio that related glycols are refined 1～1.3 is reduced to, bright
The aobvious reflux ratio less than existing special purifying ethylene glycol tower～10 being arranged on trash separator, thus makes the heat of whole polyester device
Can consume reduces～19%, and automatically controlling for purifying ethylene glycol process can be made more stable；Especially because remove impurity kettle is obtained
Quantity of steam much smaller than the first esterification mixed vapour amount, therefore the quantity of steam of remove impurity kettle operation of the change to polyester process tower
Pressure influence very little, polyester process tower stable operation, the pressure of esterifier is also relatively stable, is conducive to avoiding because of remove impurity band
The pressure transient for coming, advantageously ensures that and improves the quality of product.
Description of the drawings
Fig. 1 is the structural representation of the present invention.
Specific embodiment
Referring to Fig. 1, the material to be refined that remove impurity is related to is the liquid phase time of the mixed vapour 110 of the second esterification and polycondensation reaction
Spent glycol 120, the mixed vapour of the second esterification mainly contains ethylene glycol, also containing the water less than 10wt%, a small amount of diethylene glycol and
Acetaldehyde and a small amount of oligomer, the reuse ethylene glycol of polycondensation reaction mainly contains ethylene glycol, also the water containing～3wt%, a small amount of two
Glycol and oligomer and micro acetaldehyde.
The corresponding jacket pipes 111 of mixed vapour Jing of the second esterification deliver to trash separator（Remove impurity kettle）100, from polycondensation reaction
Reuse ethylene glycol（Liquid phase）Trash separator is sent into via ethylene glycol collecting tank（Remove impurity kettle）.
Remove impurity kettle can adopt under normal circumstances the tower reactor of jacket type（Including kettle）Deng to improve heat-insulating property, it is to avoid hold
Device encrustation, it may also be necessary to which the liquid in tower reactor is heated, to improve distillation effect of the tower bottoms in tower reactor
Really, improve the overall distilling effect of remove impurity kettle, remove impurity kettle vapo(u)rizing temperature be 180～210 DEG C, distillation pressure be 10kpa (A)
Under conditions of～100kpa (A), by mixed liquor in tower reactor（Including liquid vapour mixture）In light component such as water, ethylene glycol and ester
Compound and other heavy constituents are separated, and the glycol steam for obtaining are delivered to by the corresponding jacket pipes 141 of gaseous phase outlet Jing poly-
Ester process tower 200 mutually merges with the mixed vapour 130 of the first esterification, carries out the purification point of ethylene glycol in polyester process tower together
From.
The heating of trash separator preferably adopts external falling film type heater, the carboxylate and other impurities in trash separator and second two
The mixed solution of alcohol（Tower bottoms）Drawn by bottom, by the power that remove impurity circulating pump 152 is provided, Jing remove impurity circulation line 151
Be back to the trash separator reboiler 150 at the top of trash separator and be circulated heating, ethylene glycol that liquid phase is contained within, water and other
Light component is constantly heated evaporation, returns and the gas phase for being gathered in trash separator top is entered after trash separator, is eventually pushed to polyester work
Skill tower, liquid phase flows back to the bottom of trash separator again.
As the increase of trash separator run time, the content of the oligomer in trash separator in liquid phase are gradually stepped up, concentration is arrived
After to a certain degree, with trash separator temperature as Con trolling index, as 200～230 DEG C of trash separator Nei Wenduda, the content of ethylene glycol
Have fallen to certain degree, in order to prevent high temperature under side reaction reduce backflow ethylene glycol quality, slagging prevention, usual tower
When kettle temperature degree reaches setting value, tower bottoms needs to carry out interval deslagging, and slag liquid drains into waste collection groove through waste liquid extraction pipe 161
160。
Drawing from trash separator through the isolated gas phase light component with water and ethylene glycol as main component of trash separator
When, the spray equipment 140 at the top of trash separator is first passed through, the trapping of Jing sprays may be sprayed by impurity such as three monomers of entrainment with steam
The shower of device can connect back to spent glycol output channel 121 by corresponding pipeline, with the reuse second two of polycondensation reaction
Alcohol is spray liquid, and after spray liquid spray trash separator is flowed into, and forms the one kind for the reuse ethylene glycol that polycondensation reaction is sent into trash separator
Mode, the another way that the reuse ethylene glycol of polycondensation reaction is sent into trash separator is opened up on the wall of trash separator side with corresponding
The reuse ethylene glycol import 122 of regulating valve, and the reuse ethylene glycol output channel is connected by corresponding pipeline, after spray
Water and ethylene glycol gaseous mixture need not carry out single water and ethylene glycol is separated, but into mixing that polyester process tower and first are esterified
Close steam phase to be refined in polyester process tower together（Separate）, the refined ethylene glycol 202 formed after refining is by tower reactor
Flow out, can the light component impurity such as rear pump 230, water and acetaldehyde be set on its output channel and be steamed by polyester process column top,
Lime set collecting tank 220 is delivered to through the condensation of polyester process column top condenser 210, the part 201 in lime set is delivered at sewage
Reason, remaining Jing reflux line 223 is back to polyester process tower, and reflux ratio is controllable to 1～1.3.
The present invention has following features：
（1）The new sun proposed purifying ethylene glycol system and the main polyester process tower integrated design of polyester of original creation
The impurity removal process of ion dyeable polyester production, purifying ethylene glycol impurity removed system is not provided with independent treating column, but by trash separator
The gas phase of generation delivers to polyester process tower and carries out separating-purifying and reuse again.Compare the essence that knockout tower is separately provided on trash separator
Impurity removed system processed, present invention process can mitigate the thermic load consumption of trash separator, while the mixed vapour that trash separator is produced enters poly-
Ester process tower, can significantly mitigate the thermic load of polyester process tower as the thermal source of polyester process tower.
（2）The automatic control loop of the trash separator system of original creation design, using the heat source of remove impurity kettle as remove impurity kettle
The regulation control device of liquid level, it is ensured that the stable gas evaporation amount of trash separator, and corresponding trash separator is stable
Heating load.
（3）The impurity removal process and system of the ethylene glycol remove impurity tower of original creation design, by the steam in remove impurity kettle（Water and second two
Alcohol gaseous mixture）Deliver to polyester process tower carries out purifying ethylene glycol together with the mixed vapour of the first esterification, due to the first esterification instead
The mixed vapour amount answered much larger than remove impurity kettle draw quantity of steam, although with the viscosity of heavy constituent in ethylene glycol remove impurity kettle it is continuous
Increase, quantity of steam is changed greatly in remove impurity kettle, but in remove impurity kettle quantity of steam impact of the change to polyester process tower it is less, polyester
The stable operation of process tower, obtains the steady quality of reuse ethylene glycol.Especially because the operating pressure of polyester process tower is stablized,
The pressure disturbances to esterifier are avoided, makes the pressure of esterifier also stable, therefore, it is possible to realize more stably
Operation.Further, since the reflux ratio of polyester process tower is 1～1.3, much smaller than the second being separately provided for the second esterification mixed vapour
The tower body reflux ratio of glycol treating column up to～10, greatly reduces the energy consumption of subtractive process, due to eliminating single second two
Alcohol treating column, while also having lacked the overhead condenser and lime set collecting tank of corresponding treating column, further reduces equipment investment.
（4）The present invention can realize the refined purification purpose of the reuse ethylene glycol of cation dyeable polyester, realize product product
Matter is kept on improving, while stable, energy consumption is relatively low, be the innovation of the resource-conserving of energy-saving and emission-reduction.
（5）Due to the integrated design using trash separator and the main polyester process tower of polyester, save purifying ethylene glycol tower,
The construction investment of the equipment, pipeline and automatic control loop such as overhead condenser, lime set collecting tank and reflux pump.To produce 150000 tons per year
As a example by the cation dyeable polyester of scale, present invention process can save the construction investments such as equipment, pipeline～2,000,000 yuan.
（6）The refining and edulcoration system for being separately provided knockout tower is compared, the thermic load consumption of trash separator can be mitigated, while removing
The mixed vapour that miscellaneous device is produced enters polyester process tower, can significantly mitigate polyester process tower as the thermal source of polyester process tower
Thermic load.As a example by producing the device of 150,000 tons of scales per year, by taking the cation dyeable polyester project of 300 ton days as an example, into remove impurity system
Second esterification steam amount of system is 2850kg/h, and polycondensation reuse ethylene glycol amount is 5761kg/h.Second esterification steam water content is about
For 10wt%, polycondensation reuse ethylene glycol water content is about 2wt%.Then steam vapour amount is 400.23kg/h, according to the second being separately provided
The reflux ratio of glycol treating column is 10, and the reflux ratio of polyester process tower is calculated for 1.3, is removed with the refined of knockout tower is separately provided
Miscellaneous system process is compared, and the present invention can realize energy-conservation 6.87 × 105KJ/ ton products, signature oil 10.96kg/ ton products, signature
Coal 15.68kg/ ton products.Generally polyester product energy consumption conversion is about 57kg/ ton products for standard oil, as standard, this
The bright energy-conservation 19.2% compared with former impurity removal process.
（7）The refining and edulcoration system for being separately provided knockout tower is compared, because the present invention is not provided with treating column overhead condensation
Device, it is to avoid the consumption～208m of recirculated cooling water in condenser3/ h, energy-conservation load is about～1.1kg mark oil/ton products.
In addition to background section or separately there is special instruction outer, the second esterifier alleged by this specification is single for addition three
The esterifier of body, alleged second esterification refers to the esterification in being added with the esterification of three monomers or the second esterifier, institute
First esterifier is called to add the esterifier before three monomers, and alleged first esterification is the ester before three monomers of addition
Esterification in change or the first esterifier.
Unless otherwise specified or outside other clear and definite implications, three monomers alleged by this specification are to make polyester have cation
Dyeability and the monomer that adds, can be one or more.
The mixed vapour of the first esterification is from the mixed vapour of the first esterifier or from first alleged by this specification
The mixed vapour that esterifier is extracted out；The mixed vapour of alleged second esterification is the mixed vapour from the second esterifier
Or the mixed vapour extracted out from the second esterifier；The reuse ethylene glycol of alleged polycondensation reaction refers to the second from polycondensation unit
Glycol or the ethylene glycol extracted out from polycondensation unit（Containing water and other impurities contained therein）, generally into trash separator it
Before, it has been cooled to liquid.
Gas phase alleged by this specification refers to gaseous state or similar to gaseous state there is material or physical form, and alleged liquid phase is referred to
The material existed with liquid or similar to liquid or physical form, including the liquid containing gas and/or solid impurity and can
The solidliquid mixture of flowing.
It is used～X that numerical value is stated in this specification（Such as～3wt% ,～2,000,000 yuan）Refer to about X or X or so.
Wt% refers to mass percent in this specification.
It is disclosed by the invention it is each preferably with optional technological means, unless otherwise indicated and one preferably or can selecting technology handss
Section is outside the further restriction of another technological means, can to form some different technical schemes in any combination.
Claims (10)
1. a kind of impurity-removing method of cation dyeable polyester device, it is characterised in that the mixed vapour of the second esterification and polycondensation is anti-
The reuse ethylene glycol answered sends into trash separator remove impurity, and the trash separator is not provided with detached independent point for entering water-filling and ethylene glycol
From tower, by arranging heater, heating makes water and ethylene glycol be gas phase and be gathered in the top of trash separator inner chamber, is sending into polyester
Water and ethylene glycol gaseous mixture before process tower not to being formed enters water-filling and the separation of ethylene glycol, and oligomer to be removed with other
The impurity for going is liquid phase and is gathered in the bottom of trash separator inner chamber, and then trash separator, water are discharged by way of accomplished continuously or intermittently
Send into for water and the detached polyester process tower of ethylene glycol with ethylene glycol gaseous mixture, the mixed vapour being esterified with first is in polyester
Enter water-filling and the separation of ethylene glycol in process tower, light component impurity is steamed by the tower top of polyester process tower, the ethylene glycol of liquid phase from
The bottom of towe extraction of polyester process tower, used as the refined ethylene glycol for being back to esterifier, alleged second esterifier is to add
Plus three monomer esterifier, it is alleged second esterification refer to the ester in being added with the esterification of three monomers or the second esterifier
Change, alleged first esterifier be add three monomers before esterifier, it is alleged first esterification for addition three monomers it
Esterification in front esterification or the first esterifier, alleged three monomer adds to make polyester have cationic dye capable of dyeing
Plus monomer.
2. impurity-removing method as claimed in claim 1, it is characterised in that the trash separator using autoclave structure remove impurity kettle and set
Have trash separator reboiler, by trash separator reboiler to liquid phase heating evaporation again, be further vaporized with water contained therein and
Ethylene glycol.
3. impurity-removing method as claimed in claim 1, it is characterised in that the water and ethylene glycol gaseous mixture to the output of trash separator top
Ethylene glycol spray is carried out, three monomers and other impurities wherein carried secretly are trapped, the ethylene glycol for ethylene glycol spray is that polycondensation is anti-
The reuse ethylene glycol answered, the liquid phase after spray flows into trash separator.
4. the impurity-removing method as described in claim 1,2 or 3, it is characterised in that when trash separator is using continuously or intermittently deslagging
When, the liquid level or temperature of trash separator are controlled by the heat source of trash separator, using the primary fluid for trash separator heating
Flow is controlling the liquid level of trash separator, or realizes that the intensification of trash separator is bent using the primary fluid flow for trash separator heating
Line, so as to realize the relatively stable of trash separator liquid level, realizes the stable operation of impurity removed system.
5. a kind of knot screen of cation dyeable polyester device, it is characterised in that including trash separator and for water and ethylene glycol point
From polyester process tower, the trash separator is not provided with for water and the detached independent separate tower of ethylene glycol, the trash separator connection
The mixed vapour output channel of the second esterification and the reuse ethylene glycol output channel of polycondensation reaction, thus access the mixed of the second esterification
Close the reuse ethylene glycol of steam and polycondensation reaction and carry out heating evaporation so as in water and ethylene glycol be gas phase, be gathered in and remove
The top of miscellaneous device inner chamber, oligomer and other impurity that should be removed are liquid phase and are gathered in the bottom of trash separator inner chamber, described to remove
Mixed gas outlet is provided with the top of miscellaneous device, bottom is provided with slag-drip opening, the mixed vapour of the esterification of polyester process tower connection first
The mixed gas outlet of output channel and the trash separator, accesses the mixed vapour of the first esterification and the water and second two of trash separator output
Alcohol gaseous mixture simultaneously carries out heating evaporation so as in light component impurity be gas phase, ethylene glycol is liquid phase, the polyester process tower
Tower top is provided with steam outlet, and bottom of towe is provided with refined ethylene glycol outlet, and alleged second esterifier is the ester for adding three monomers
Change reactor, alleged second esterification refers to the esterification in being added with the esterification of three monomers or the second esterifier, alleged first
Esterifier is to add the esterifier before three monomers, and alleged first esterification is the esterification or the before three monomers of addition
Esterification in one esterifier, the monomer that alleged three monomer adds to make polyester have cationic dye capable of dyeing.
6. knot screen as claimed in claim 5, it is characterised in that the trash separator using autoclave structure remove impurity kettle and set
There is trash separator reboiler, the trash separator reboiler is located at the top of the trash separator, its top is provided with material inlet, and bottom sets
The material outlet for having material outlet, the trash separator reboiler directly connects described by the respective openings at the top of the trash separator
The inner chamber of trash separator, the material inlet of the trash separator reboiler connects the deslagging of the trash separator by trash separator circulating line
Mouthful, the trash separator circulating line is provided with trash separator circulating pump, boils again positioned at the trash separator circulating pump and the trash separator
Waste liquid extraction pipe is connected with the trash separator circulating line between the material inlet of device, the waste liquid produces the outer termination of pipe
Enter waste collection groove, periodically or continuously the excessive liquid phase of viscosity in trash separator is entered into the waste collection groove.
7. knot screen as claimed in claim 5, it is characterised in that be provided with ethylene glycol at the mixed gas outlet of the trash separator
Spray equipment, the ethylene glycol spray device is provided with the shower with nozzle, the injection direction of the nozzle be it is reverse, i.e., with
The outflow of water and ethylene glycol gaseous mixture is in opposite direction, and the shower connects the reuse ethylene glycol outlet tube of the polycondensation reaction
Thus road, constituted using the reuse ethylene glycol of polycondensation reaction as the ethylene glycol of spray and the trash separator connection polycondensation anti-
A kind of mode of the reuse ethylene glycol output channel answered, the side of the trash separator is provided with reuse ethylene glycol import, the reuse
Ethylene glycol import connects the reuse ethylene glycol output channel of the polycondensation reaction and is provided with regulating valve, thus constitutes the trash separator
Connect the another way of the reuse ethylene glycol output channel of the polycondensation reaction.
8. the knot screen as described in claim 6, it is characterised in that the trash separator is provided with external or built-in plus hot charging
Put, the heater is provided with primary fluid conveyance conduit.
9. the knot screen as described in claim 7, it is characterised in that the trash separator is provided with external or built-in plus hot charging
Put, the heater is provided with primary fluid conveyance conduit.
10. knot screen as claimed in claim 8, it is characterised in that be additionally provided with impurity removed system controller, the trash separator sets
Have the signal output of liquid level sensor and/or temperature sensor, the liquid level sensor and/or temperature sensor by wired or
Wireless mode accesses the impurity removed system controller, and the waste liquid extraction pipe or trash separator circulating line are provided with deslagging flow
Meter, the signal output of the deslagging effusion meter accesses impurity removed system controller, the primary fluid by wired or wireless way
Conveyance conduit is provided with primary fluid regulating valve, the corresponding control signal of the impurity removed system controller be input into respectively it is described once
The control end of heating agent regulating valve and the trash separator circulating pump.
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| CN201510503526.6A CN105061144B (en) | 2015-08-17 | 2015-08-17 | Impurity removal method and impurity removal system for cationic dyeable polyester device |
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| CN201510503526.6A CN105061144B (en) | 2015-08-17 | 2015-08-17 | Impurity removal method and impurity removal system for cationic dyeable polyester device |
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| US10124330B2 (en) * | 2011-06-14 | 2018-11-13 | Equinor Energy As | Method and apparatus for the removal of polyvalent cations from mono ethylene glycol |
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